Preparation process of electromagnetic protection and magnetic health care fabric
Nanoscale magnetic CoFe2O4@C fibers were prepared by electrospinning with graphene coated by sol-gel method and CVD method, which solved the problems of inconsistent health care effects and electromagnetic radiation hazards of magnetic textiles, and realized the preparation of highly efficient electromagnetic protection and magnetic health care fabrics.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- HEYE HEALTH TECH CO LTD
- Filing Date
- 2023-06-05
- Publication Date
- 2026-04-14
AI Technical Summary
In the existing technology, the health care mechanism of magnetic textiles is inconsistent, and with the increase of industrial equipment, the harm of electromagnetic radiation to the human body is becoming increasingly serious. There is a lack of effective methods for preparing electromagnetic protective magnetic health care fabrics.
Iron-cobalt ferrite gel was prepared by sol-gel method, graphene was coated by CVD method, and nano-magnetic CoFe2O4@C fibers were prepared by electrospinning. Combined with spinning and weaving processes, electromagnetic protective and magnetic health care fabric was prepared.
It achieves effective protection against electromagnetic radiation, enhances the fabric's puncture resistance, moisture permeability, and magnetic durability, and improves the magnetic health benefits.
Smart Images

Figure CN116676700B_ABST
Abstract
Description
Technical Field
[0001] This invention specifically relates to a preparation process of an electromagnetic protection magnetic health care fabric, belonging to the technical field of production process for wave-absorbing magnetic health care products. Background Technology
[0002] The meaning of health care refers to the comprehensive measures taken to protect and improve human health and prevent and treat diseases.
[0003] Magnetic fibers and their products, possessing magnetic therapy effects, are often classified as health textiles. Currently, the mechanisms underlying the health benefits of magnetic textiles are diverse and lack a unified conclusion. For example, a magnetic field acting on the human body can influence the orientation of bioelectricity and the magnetic moments of biological macromolecules, causing a series of physicochemical reactions known as magnetobiological effects. These include increased cell membrane permeability, promoting the exchange of substances between intracellular and extracellular spaces, and affecting nerve excitability and enzyme activity. Magnetic fibers and their fabrics contain permanent magnets, which can continuously supply a magnetic field to the outside world. Upon contact with the human body, this activates cellular metabolism and promotes microcirculation. Magnetic fibers and their fabrics can supply a constant magnetic field. Clinically, static magnetic fields can promote the proliferation of osteoblasts and skeletal muscle cells, accelerate fracture healing, inhibit and delay the onset of hypertension, protect the cardiovascular system, enhance the deformability of red blood cells, reduce blood viscosity, and inhibit the development of hyperglycemia in diabetic organisms. Furthermore, human blood is rich in iron ions and electrolytes, as well as many charged molecules and ions. When blood moves in a magnetic field, these iron ions and electrolytes are subjected to forces that generate heat, causing the blood vessels containing these iron ions and electrolytes to dilate. This dilation allows more blood to flow through, thus promoting blood circulation and enhancing the supply of nutrients and oxygen to local tissues. Additionally, the weakening of the Earth's magnetic field and modern industrial processes have disrupted the magnetic field balance around the human body, necessitating the replenishment and regulation of this balance. Magnetic fiber products can effectively improve this situation.
[0004] With the rapid development of social technology and the rapid increase in industrial equipment, people are now surrounded by various electromagnetic devices, and electromagnetic radiation is becoming increasingly harmful to the human body. As a result, people are paying more attention to how to reduce electromagnetic radiation. Electromagnetic wave absorbing fabrics and textiles made of nano-magnetic materials that can absorb waves have a good electromagnetic wave absorbing effect and can provide a good electromagnetic protection effect for the human body. Therefore, electromagnetic protection and health care fabrics are becoming an important research object. Summary of the Invention
[0005] In order to overcome the above-mentioned technical problems existing in the existing technical field, the purpose of this invention is to provide a preparation process for electromagnetic protective magnetic health care fabric, so as to promote its development and application.
[0006] The present invention provides a preparation process for an electromagnetic protection and health care fabric, comprising the following steps:
[0007] Step (1) Preparation of iron cobalt ferrite gel
[0008] Weigh out specific amounts of Co(NO3)2·6H2O and Fe(NO3)3·9H2O, and measure out a specific amount of deionized water, then place them together in a clamped beaker and stir in a water bath at a specific temperature. Add a specific amount of citric acid and continue stirring, then add a specific amount of ammonia to adjust the pH of the solution. Adjust the water bath to a suitable temperature and continue stirring until the solution becomes a sol. Then pour the resulting sol into a beaker, transfer it to a forced-air drying oven, and dry it at a specific temperature to obtain an iron-cobalt ferrite gel.
[0009] Step (2) Preparation of iron-cobalt ferrite nanopowder
[0010] After the iron-cobalt ferrite gel is finely ground, it is placed in a crucible and calcined in a box-type resistance furnace at a certain temperature for a period of time to obtain iron-cobalt ferrite CoFe2O4 nanopowder.
[0011] Step (3) CVD coating of graphene
[0012] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing iron-cobalt ferrite (CoFe₂O₄) nanoparticles was placed inside a quartz tube and heated to a certain temperature. Then, acetylene was introduced at a controlled flow rate and the reaction proceeded for a period of time. Next, the temperature was appropriately increased, and the product was held at this temperature in an argon atmosphere for a period of time. The reaction system was then slowly cooled in an argon atmosphere until a suitable temperature was reached, at which point the argon gas supply was turned off, and the system was allowed to cool slowly to room temperature in air. The product was collected, soaked in hydrochloric acid for a period of time, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe₂O₄@C nanoparticles.
[0013] Step (4) Preparation of nano-magnetic CoFe2O4@C fibers
[0014] Nano-magnetic CoFe2O4@C fibers were prepared by electrospinning. An appropriate amount of nano-magnetic CoFe2O4@C particles were ultrasonically dispersed in polyvinylpyrrolidone (PVP) and magnetically stirred for a period of time to prepare a spinning solution. The spinning solution was then sprayed out of the spinneret through an electrostatic nozzle and entered a high-voltage electrostatic field, and finally deposited in a collector to become nano-magnetic CoFe2O4@C fibers.
[0015] Step (5) Spinning and weaving
[0016] The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving.
[0017] Preferably, step (1) of preparing the iron-cobalt ferrite gel involves weighing 6-8 g of Co(NO3)2·6H2O and 19-22 g of Fe(NO3)3·9H2O, and measuring 40-60 mL of deionized water, placing them together in a clamped beaker, and stirring in a water bath at 50-70°C for 1-3 hours. Then, 5-20 mL of citric acid is added, and stirring continues for 3-7 hours. A certain amount of ammonia is then added to adjust the pH of the solution to 2.5-4.5. The water bath temperature is adjusted to 60-75°C, and stirring continues until the solution becomes a sol. The resulting sol is then poured into a beaker and transferred to a forced-air drying oven at 200-300°C for drying to obtain the iron-cobalt ferrite gel.
[0018] This method uses the sol-gel method to prepare iron-cobalt ferrite gels. Its advantages lie in its ability to fully disperse Co(NO3)2·6H2O and Fe(NO3)3·9H2O in the solvent, achieving molecular-level homogeneity in a short time. The method is simple, efficient, and easy to produce, yielding highly complete and pure iron-cobalt ferrite crystal nuclei. A certain amount of citric acid is added during the process to act as a complexing agent, facilitating the dispersion of cobalt and iron ions in the solvent. This provides higher local energy during subsequent heat treatment, promoting crystal formation. Furthermore, the added citric acid enhances the magnetic properties of the product. During the preparation process, the pH value needs to be adjusted to 2.5–4.5 to maintain an acidic environment, which is to inhibit Fe... 3+ The hydrolysis ensures that the final crystallized product contains no other impurities.
[0019] Preferably, step (2) involves preparing iron cobalt ferrite nanopowder by grinding the iron cobalt ferrite gel into a crucible and calcining it in a box-type resistance furnace at a temperature of 700~900℃ for 2~4h to obtain iron cobalt ferrite CoFe2O4 nanopowder.
[0020] When preparing cobalt iron ferrite nanopowder, the cobalt iron ferrite gel needs to be finely ground in order to have a larger heating surface area during the subsequent calcination process, which will accelerate the formation of cobalt iron ferrite CoFe2O4 nanopowder and make the particle size of the formed CoFe2O4 nanopowder more uniform.
[0021] Preferably, step (3) of CVD coating of graphene involves the synthesis of graphene by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 1-3 g of iron-cobalt ferrite CoFe2O4 nanoparticles is placed inside a quartz tube, and the temperature is raised to 350-450°C. Then, acetylene (99.9-99.99% by volume) is introduced at a flow rate of 25-45 mL / min, and the reaction is allowed to proceed for 1-3 hours. Next, the temperature is appropriately increased to 600-700°C, and the product is kept at this temperature in an argon atmosphere for 2-3 hours. Then, the reaction system is slowly cooled in an argon atmosphere until it reaches 300-350°C, at which point the argon gas source is turned off, and the reaction system is slowly cooled to room temperature in the air. The product is collected, soaked in hydrochloric acid for 1-2 hours, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe2O4@C nanoparticles.
[0022] In the CVD coating of graphene, the first step of heating to 350-450℃ serves as a preheating process, allowing the CoFe2O4 magnetic nanoparticles to slowly and fully contact acetylene, increasing the contact area. Simultaneously, the CoFe2O4 magnetic nanoparticles act as a catalyst, accelerating the acetylene cracking process while increasing the contact area. Heating the initial reaction to 350-450℃ also prevents the generated graphene from agglomerating on the surface of the magnetic nanoparticles, which would result in poor coating. After the reaction, soaking in hydrochloric acid removes the carrier and other residual impurities, improving product purity.
[0023] Preferably, step (4) involves preparing nano-magnetic CoFe2O4@C fibers by electrospinning. This includes taking 2-3g of nano-magnetic CoFe2O4@C particles, ultrasonically dispersing them in 20-30mL of polyvinylpyrrolidone (PVP), and preparing a spinning solution by magnetic stirring for 2-3 hours. The spinning solution is then sprayed out of the spinneret through an electrostatic nozzle and enters a high-voltage electrostatic field, finally depositing in a collector to become nano-magnetic CoFe2O4@C fibers. The main parameters are: spinneret specification: SPN1500×0.12 mm, and spinning speed: 10-20cm / s.
[0024] By utilizing ultra-high electrostatics, the spinning solution ejected from the spinneret is formed into nanofibers under the action of an electric field. This method features simple preparation, fast speed, and easy collection of nanofibers on the collector, resulting in a high yield.
[0025] Preferably, in step (5), spinning and weaving, the prepared nano-magnetic CoFe2O4@C fiber bundles are processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in this process are: blending ratio 30:30~60:60, repeated 2~3 times, blending weight 3~4 g / m, number of rovings 4~8, roving weight 0.3~1.0 g / m, and spinning weight 1~2 g / 100 m.
[0026] Because the prepared nanofibers have certain characteristics such as being free of impurities and having a relatively long length, they need to undergo a carding process. During the carding process, the main function is to comb and mix the fibers to enlarge the working area spacing, reduce fiber damage, and reduce fiber deposition. The fibers are then transferred before the subsequent spinning operation.
[0027] The electromagnetic protective and health care fabric prepared using nano-magnetic CoFe2O4@C fiber bundles according to this invention has the advantages of protecting the human body, reducing electromagnetic radiation from various electronic devices, and providing magnetic health care benefits. Attached Figure Description
[0028] Figure 1 This is a process flow diagram for the preparation of an electromagnetic protective and health care fabric. Detailed Implementation
[0029] Example 1
[0030] The present invention provides a preparation process for an electromagnetic protection and health care fabric, comprising the following steps:
[0031] Step (1) Preparation of iron cobalt ferrite gel
[0032] Weigh out 6g of Co(NO3)2·6H2O and 19g of Fe(NO3)3·9H2O, and add 40mL of deionized water to a clamped beaker. Stir in a 50℃ water bath for 1 hour. Add 5mL of citric acid and continue stirring for 3 hours. Then add a certain amount of ammonia to adjust the pH of the solution to 4.5. Adjust the water bath temperature to 60℃ and continue stirring until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a forced-air drying oven to dry at 200℃ to obtain an iron-cobalt ferrite gel.
[0033] Step (2) Preparation of iron-cobalt ferrite nanopowder
[0034] The cobalt iron ferrite gel was finely ground and placed in a crucible, which was then placed in a box-type resistance furnace and calcined at 700°C for 2 hours to obtain cobalt iron ferrite CoFe2O4 nanopowder.
[0035] Step (3) CVD coating of graphene
[0036] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 1 g of iron-cobalt ferrite (CoFe₂O₄) nanoparticles was placed inside a quartz tube, and the temperature was raised to 350°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 25 mL / min, and the reaction was allowed to proceed for 1 h. Next, the temperature was appropriately increased to 600°C, and the product was held at this temperature in an argon atmosphere for 2 h. The reaction system was then slowly cooled in an argon atmosphere until it reached 300°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 1 h, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe₂O₄@C nanoparticles.
[0037] Step (4) Preparation of nano-magnetic CoFe2O4@C fibers
[0038] Nanoscale magnetic CoFe2O4@C fibers were prepared by electrospinning. 2g of nanoscale magnetic CoFe2O4@C particles were ultrasonically dispersed in 20mL of polyvinylpyrrolidone (PVP), and the mixture was magnetically stirred for 2 hours to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic CoFe2O4@C fibers in a collector. The main parameters were: spinneret specification: SPN1500×0.12 mm; spinning speed: 10 cm / s.
[0039] Step (5) Spinning and weaving
[0040] The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: a blending ratio of 30:30, repeated twice, a blending sliver weight of 3 g / m, 4 slivers combined, a roving weight of 0.3 g / m, and a spinning weight of 1 g / 100 m.
[0041] Example 2
[0042] Step (1) Preparation of iron cobalt ferrite gel
[0043] Weigh out 6.5 g of Co(NO3)2·6H2O and 20 g of Fe(NO3)3·9H2O, and add 40 mL of deionized water to a clamped beaker. Stir in a water bath at 55 °C for 1.5 h. Add 10 mL of citric acid and continue stirring for 4 h. Then add a certain amount of ammonia to adjust the pH of the solution to 4.0. Adjust the water bath temperature to 65 °C and continue stirring until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a drying oven at 225 °C to dry, obtaining an iron-cobalt ferrite gel.
[0044] Step (2) Preparation of iron-cobalt ferrite nanopowder
[0045] The cobalt iron ferrite gel was finely ground and placed in a crucible, then calcined in a box-type resistance furnace at 725°C for 2.5 hours to obtain cobalt iron ferrite CoFe2O4 nanopowder.
[0046] Step (3) CVD coating of graphene
[0047] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 2g of iron-cobalt ferrite (CoFe₂O₄) nanoparticles was placed inside a quartz tube, and the temperature was raised to 375°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 30mL / min, and the reaction was allowed to proceed for 1 hour. Next, the temperature was appropriately increased to 625°C, and the product was held at this temperature in an argon atmosphere for 2 hours. The reaction system was then slowly cooled in an argon atmosphere until it reached 300°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 1 hour, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe₂O₄@C nanoparticles.
[0048] Step (4) Preparation of nano-magnetic CoFe2O4@C fibers
[0049] Nanoscale magnetic CoFe2O4@C fibers were prepared by electrospinning. 2.2 g of nanoscale magnetic CoFe2O4@C particles were ultrasonically dispersed in 20 mL of polyvinylpyrrolidone (PVP) and magnetically stirred for 2 h to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic CoFe2O4@C fibers in a collector. The main parameters are: spinneret specification: SPN1500×0.13 mm; spinning speed: 13 cm / s.
[0050] Step (5) Spinning and Weaving
[0051] The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: blending ratio 40:40, repeated twice, blending sliver weight 3.2 g / m, number of pliers 5, roving weight 0.6 g / m, and spinning weight 1.2 g / 100 m.
[0052] Example 3
[0053] Step (1) Preparation of iron cobalt ferrite gel
[0054] Weigh out 7g of Co(NO3)2·6H2O and 21g of Fe(NO3)3·9H2O, and add 50mL of deionized water to a clamped beaker. Stir in a 60℃ water bath for 2.0h. Add 15mL of citric acid and continue stirring for 3.5h. Then add a certain amount of ammonia to adjust the pH of the solution to 3.5. Adjust the water bath temperature to 70℃ and stir continuously until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a forced-air drying oven to dry at 250℃ to obtain an iron-cobalt ferrite gel.
[0055] Step (2) Preparation of iron-cobalt ferrite nanopowder
[0056] The cobalt iron ferrite gel was finely ground and placed in a crucible, then calcined in a box-type resistance furnace at 750°C for 2.5 hours to obtain cobalt iron ferrite CoFe2O4 nanopowder.
[0057] Step (3) CVD coating of graphene
[0058] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 2.4 g of iron-cobalt ferrite (CoFe₂O₄) nanoparticles was placed inside a quartz tube, and the temperature was raised to 400°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 35 mL / min, and the reaction was allowed to proceed for 1.5 h. The temperature was then appropriately increased to 650°C, and the product was held at this temperature in an argon atmosphere for 2 h. The reaction system was then slowly cooled in an argon atmosphere until it reached 325°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 1.5 h, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe₂O₄@C nanoparticles.
[0059] Step (4) Preparation of nano-magnetic CoFe2O4@C fibers
[0060] Nanoscale magnetic CoFe2O4@C fibers were prepared by electrospinning. 2.4 g of nanoscale magnetic CoFe2O4@C particles were ultrasonically dispersed in 25 mL of polyvinylpyrrolidone (PVP) and magnetically stirred for 2.5 h to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic CoFe2O4@C fibers in a collector. The main parameters were: spinneret specification: SPN1600×0.13 mm; spinning speed: 15 cm / s.
[0061] Step (5) Spinning and Weaving
[0062] The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: a blending ratio of 50:50, repeated 3 times, a blending sliver weight of 3.4 g / m, 6 filaments combined, a roving weight of 0.8 g / m, and a spinning weight of 1.5 g / 100 m.
[0063] Example 4
[0064] Step (1) Preparation of iron cobalt ferrite gel
[0065] Weigh out 7.5 g of Co(NO3)2·6H2O and 22 g of Fe(NO3)3·9H2O, and add 50 mL of deionized water to a clamped beaker. Stir in a water bath at 65 °C for 2.0 h. Add 15 mL of citric acid and continue stirring for 3.5 h. Then add a certain amount of ammonia to adjust the pH of the solution to 3.0. Adjust the water bath temperature to 75 °C and stir continuously until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a drying oven at 275 °C to dry, obtaining an iron-cobalt ferrite gel.
[0066] Step (2) Preparation of iron-cobalt ferrite nanopowder
[0067] The cobalt iron ferrite gel was finely ground and placed in a crucible, then placed in a box-type resistance furnace and calcined at 775°C for 3.0 h to obtain cobalt iron ferrite CoFe2O4 nanopowder.
[0068] Step (3) CVD coating of graphene
[0069] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 2.7 g of iron-cobalt ferrite (CoFe₂O₄) nanoparticles was placed inside a quartz tube, and the temperature was raised to 400°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 40 mL / min, and the reaction was allowed to proceed for 1 h. Next, the temperature was appropriately increased to 675°C, and the product was held at this temperature in an argon atmosphere for 2 h. The reaction system was then slowly cooled in an argon atmosphere until it reached 345°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 2.0 h, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe₂O₄@C nanoparticles.
[0070] Step (4) Preparation of nano-magnetic CoFe2O4@C fibers
[0071] Nanoscale magnetic CoFe2O4@C fibers were prepared by electrospinning. 3.0 g of nanoscale magnetic CoFe2O4@C particles were ultrasonically dispersed in 30 mL of polyvinylpyrrolidone (PVP) and magnetically stirred for 3 h to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic CoFe2O4@C fibers in a collector. The main parameters were: spinneret specification: SPN1600×0.13 mm; spinning speed: 17 cm / s.
[0072] Step (5) Spinning and weaving
[0073] The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: a blending ratio of 60:60, repeated 3 times, a blending sliver weight of 3.7 g / m, 7 filaments combined, a roving weight of 0.9 g / m, and a spinning weight of 1.7 g / 100 m.
[0074] Comparative Example 1
[0075] Step (1) Preparation of iron barium ferrite gel
[0076] Weigh out 6g of Ba(NO3)2·4H2O and 19g of Fe(NO3)3·9H2O, and add 40mL of deionized water to a clamped beaker. Stir in a 50℃ water bath for 1 hour. Add 5mL of citric acid and continue stirring for 3 hours. Then add a certain amount of ammonia to adjust the pH of the solution to 4.5. Adjust the water bath temperature to 60℃ and continue stirring until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a forced-air drying oven to dry at 200℃ to obtain iron barium ferrite gel.
[0077] Step (2) Preparation of barium iron ferrite nanopowder
[0078] The iron barium ferrite gel was finely ground and placed in a crucible, and then calcined in a box-type resistance furnace at 700°C for 2 hours to obtain iron cobalt ferrite BaFe2O4 nanopowder.
[0079] Step (3) CVD coating of graphene
[0080] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 1 g of iron-cobalt ferrite BaFe₂O₄ nanoparticles was placed inside a quartz tube, and the temperature was raised to 350°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 25 mL / min, and the reaction was allowed to proceed for 1 h. Next, the temperature was appropriately increased to 600°C, and the product was held at this temperature in an argon atmosphere for 2 h. The reaction system was then slowly cooled in an argon atmosphere until it reached 300°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 1 h, and then rinsed with deionized water to obtain graphene-coated magnetic BaFe₂O₄@C nanoparticles.
[0081] Step (4) Preparation of nano-magnetic BaFe2O4@C fibers
[0082] Nanoscale magnetic BaFe2O4@C fibers were prepared by electrospinning. 2g of nanoscale magnetic BaFe2O4@C particles were ultrasonically dispersed in 20mL of polyvinylpyrrolidone (PVP), and the mixture was magnetically stirred for 2 hours to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic BaFe2O4@C fibers in a collector. The main parameters were: spinneret specification: SPN1500×0.12 mm; spinning speed: 10 cm / s.
[0083] Step (5) Spinning and Weaving
[0084] The prepared nano-magnetic BaFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: a blending ratio of 30:30, repeated twice, a blending sliver weight of 3 g / m, 4 slivers combined, a roving weight of 0.3 g / m, and a spinning weight of 1 g / 100 m.
[0085] Comparative Example 2
[0086] Step (1) Preparation of iron barium ferrite gel
[0087] Weigh out 6.5 g of Ba(NO3)2·4H2O and 22 g of Fe(NO3)3·9H2O, and add 40 mL of deionized water to a clamped beaker. Stir in a 50°C water bath for 1.5 h. Add 15 mL of citric acid and continue stirring for 3 h. Then add a certain amount of ammonia to adjust the pH of the solution to 3.5. Adjust the water bath temperature to 70°C and continue stirring until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a forced-air drying oven to dry at 250°C to obtain iron barium ferrite gel.
[0088] Step (2) Preparation of barium iron ferrite nanopowder
[0089] The iron barium ferrite gel was finely ground and placed in a crucible, and then calcined in a box-type resistance furnace at 750°C for 2 hours to obtain iron cobalt ferrite BaFe2O4 nanopowder.
[0090] Step (3) CVD coating of graphene
[0091] The product was synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 1.5 g of iron-cobalt ferrite BaFe2O4 nanoparticles was placed inside a quartz tube, and the temperature was raised to 350°C. Then, acetylene (99.99% by volume) was introduced at a flow rate of 35 mL / min, and the reaction was allowed to proceed for 1 h. The temperature was then appropriately increased to 700°C, and the product was held at this temperature in an argon atmosphere for 2 h. The reaction system was then slowly cooled in an argon atmosphere until it reached 325°C, at which point the argon gas supply was turned off, and the system was allowed to slowly cool to room temperature in air. The product was collected, soaked in hydrochloric acid for 1 h, and then rinsed with deionized water to obtain graphene-coated magnetic BaFe2O4@C nanoparticles.
[0092] Step (4) Preparation of nano-magnetic BaFe2O4@C fibers
[0093] Nanoscale magnetic BaFe2O4@C fibers were prepared by electrospinning. 2.5 g of nanoscale magnetic BaFe2O4@C particles were ultrasonically dispersed in 25 mL of polyvinylpyrrolidone (PVP) and magnetically stirred for 3 h to prepare a spinning solution. The spinning solution was then ejected from the spinneret through an electrostatic nozzle and introduced into a high-voltage electrostatic field, ultimately depositing as nanoscale magnetic BaFe2O4@C fibers in a collector. The main parameters were: spinneret specification: SPN1500×0.12 mm; spinning speed: 15 cm / s.
[0094] Step (5) Spinning and weaving
[0095] The prepared nano-magnetic BaFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through processes such as wool spinning, carding, drawing, roving, spinning, winding, and weaving. The main parameters in the process were: a blending ratio of 50:50, repeated 3 times, a blending sliver weight of 3.5 g / m, 7 filaments combined, a roving weight of 0.8 g / m, and a spinning weight of 1.6 g / 100 m.
[0096] The electromagnetic protective and magnetic health care fabric samples prepared in Examples 1 to 4 and Comparative Examples 1 and 2 were subjected to performance tests. The specific testing methods are as follows:
[0097] Breakthrough test
[0098] Using an INstron 3365 material testing machine, the fabric samples were cut into circular pieces with a diameter of 45±0.5mm. Five pieces of each type of fabric were cut and tested according to GB / T 19976-2005 "Determination of bursting strength of textiles - steel ball method". Multiple tests were conducted and the average value was taken.
[0099] Moisture permeability test
[0100] The Fx3150 fully automatic fabric moisture permeability tester manufactured by Textest GmbH, Switzerland, was used. The samples were cut into circular pieces with a diameter of 70 mm, and three pieces were cut for each type of fabric. The test was carried out in accordance with GB / T 12704.2-2009 "Textiles - Test Methods for Moisture Permeability of Fabrics - Part 2 - Evaporation Method". Multiple tests were conducted and the average value was taken.
[0101] Wave absorption performance test
[0102] The dielectric constant and permeability of different fabric samples were tested using an AV3296 vector network analyzer. The RL value was then calculated based on the measured electromagnetic parameters; a smaller RL value indicates better wave absorption capability. Multiple tests were conducted, and the average value was taken.
[0103] Magnetic durability test
[0104] Following GB / T 8629-2001 "Home Washing and Drying Procedures for Textile Testing", samples were cut into 30cm × 30cm pieces, with seven pieces for each type of fabric. A 100cm × 100cm piece of pure cotton woven fabric was used as a wash companion. All samples were washed, laid flat, and air-dried. The magnetic induction intensity of the magnetic fabric surface was measured using a Swiss Metrolab magnetic field strength tester before and after each wash. Multiple experiments were conducted, and the average value was calculated.
[0105] Table 1. Test results of bursting performance
[0106]
[0107] As shown in Table 1, Examples 1 to 4 all exhibit higher burst resistance than Comparative Examples 1 and 2, reflecting the requirements for burst resistance in composite garment textiles. Comparing Examples 1 to 4 reveals that the higher the content of magnetic fibers, the better the burst resistance of the fabric. This is because magnetic fibers enhance the toughness and strength of other fabric fibers during the spinning process, resulting in better mechanical strength of the woven yarn. In contrast, the comparative examples, due to the presence of more defects within the magnetic fibers in barium iron ferrite compared to cobalt iron ferrite, exhibited lower burst resistance compared to the examples.
[0108] Table 2. Test results of moisture permeability for each embodiment and comparative example.
[0109]
[0110] Table 2 shows that, comparing Examples 1 to 4 with Comparative Examples 1 and 2, the moisture permeability of the examples is greater than that of the comparative examples, meeting the moisture permeability requirements for everyday textiles. Fabric moisture permeability refers to the ability of water vapor to pass through the fabric. Different fabrics may evaporate different amounts of water in the same time period; the greater the amount of water evaporated, the better the fabric's moisture permeability. The experimental results show that as the content of nano-magnetic fibers increases, the difference in moisture permeability is not significant, greatly improving the convenience and applicability of textiles for everyday use. The comparative examples used barium iron ferrite as the main magnetic source for the nano-magnetic fibers. Due to its numerous surface defects and high moisture absorption, its moisture permeability decreased.
[0111] Table 3. Test results of microwave absorption performance of each embodiment and comparative example.
[0112]
[0113] Table 3 shows that the microwave absorption capabilities of Comparative Examples 1 to 4 are stronger than those of Comparative Examples 1 and 2. This is because cobalt, an element in the iron-cobalt ferrite used in these examples, is a transition metal in the periodic table and has more high-energy electrons than barium, a main metal. Therefore, iron-cobalt ferrite possesses stronger dielectric constant, electromagnetic loss, and dielectric loss properties. The lower the measured RL value, the better its microwave absorption performance. The magnetic health fabric prepared from this fabric can better protect the human body from the harmful effects of external electromagnetic radiation, thus protecting human health.
[0114] Table 4 Magnetic Durability Test Results
[0115]
[0116] As shown in Table 4, all embodiments and comparative examples exhibit good magnetic durability. The differences between the maximum and average values before and after washing are not significant. This is because both iron-cobalt ferrite and iron-barium ferrite are permanent magnets with strong magnetic durability. Since iron-cobalt ferrite has a higher magnetic strength than iron-barium ferrite, it provides better magnetic health benefits to the human body when prepared into magnetic health fabrics. Furthermore, the electromagnetic protective magnetic health fabrics and products prepared using this method produce less fuzz on the fabric surface before and after washing, and the loss of magnetic fiber content is minimal, which also improves the magnetic durability of the fabric and extends the product's lifespan.
[0117] This specific embodiment is merely an explanation of the present invention and is not intended to limit the present invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but as long as they are within the scope of the claims of the present invention, they are protected by patent law.
Claims
1. A preparation process for an electromagnetic protective magnetic health care fabric, characterized in that: Step (1) Preparation of iron cobalt ferrite gel Weigh out a certain amount of Co(NO3)2·6H2O and Fe(NO3)3·9H2O, and measure a certain amount of deionized water, and place them together in a clamped beaker. Stir in a water bath at a certain temperature. Add a certain amount of citric acid and continue stirring. Then add a certain amount of ammonia to adjust the pH of the solution. Adjust the water bath to a suitable temperature and stir until the solution becomes a sol. Pour the resulting sol into a beaker and transfer it to a forced-air drying oven to dry at a certain temperature to obtain iron-cobalt ferrite gel. Step (2) Preparation of iron-cobalt ferrite nanopowder After the iron-cobalt ferrite gel is finely ground, it is placed in a crucible and calcined in a box-type resistance furnace at a certain temperature for a period of time to obtain iron-cobalt ferrite CoFe2O4 nanopowder. Step (3) CVD coating of graphene The product is synthesized by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing iron-cobalt ferrite (CoFe2O4) nanoparticles is placed inside a quartz tube and heated to a certain temperature. Then, acetylene is introduced at a specific flow rate and the reaction is allowed to proceed for a period of time. Next, the temperature is appropriately increased, and the product is kept at this temperature in an argon atmosphere for a period of time. Then, the reaction system is slowly cooled in an argon atmosphere until a suitable temperature is reached, at which point the argon gas source is turned off, and the reaction system is slowly cooled to room temperature in air. The product is collected, soaked in hydrochloric acid for a period of time, and then rinsed with deionized water to obtain graphene-coated magnetic CoFe2O4@C nanoparticles. Step (4) Preparation of nano-magnetic CoFe2O4@C fibers Nano-magnetic CoFe2O4@C fibers were prepared by electrospinning. An appropriate amount of nano-magnetic CoFe2O4@C particles were ultrasonically dispersed in polyvinylpyrrolidone (PVP) and magnetically stirred for a period of time to prepare a spinning solution. The spinning solution was then sprayed out of the spinneret through an electrostatic nozzle and entered a high-voltage electrostatic field, and finally deposited in a collector to become nano-magnetic CoFe2O4@C fibers. Step (5) Spinning and weaving The prepared nano-magnetic CoFe2O4@C fiber bundles were processed into electromagnetic protective and health care fabrics through wool, carding, drawing, roving, spinning, winding, and weaving processes.
2. The preparation process of an electromagnetic protective magnetic health care fabric according to claim 1, characterized in that: Step (1) Preparation of iron cobalt ferrite gel: Weigh 6-8g of Co(NO3)2·6H2O and 19-22g of Fe(NO3)3·9H2O and measure 40-60mL of deionized water and put them into a clamped beaker. Stir in a water bath at 50-70℃ for 1-3h; add 5-20mL of citric acid and continue stirring for 3-7h. Then add a certain amount of ammonia to adjust the pH of the solution to 2.5-4.5; adjust the water bath to 60-75℃ and stir until the solution becomes a sol; then pour the obtained sol into a beaker and transfer it to a forced-air drying oven at 200-300℃ to dry, and obtain iron cobalt ferrite gel.
3. The preparation process of an electromagnetic protective magnetic health care fabric according to claim 2, characterized in that: Step (2) Preparation of iron cobalt ferrite nanopowder includes grinding the iron cobalt ferrite gel into a crucible and placing it in a box-type resistance furnace at a temperature of 700~900℃ for 2~4h to obtain iron cobalt ferrite CoFe2O4 nanopowder.
4. The preparation process of an electromagnetic protective magnetic health care fabric according to claim 3, characterized in that: Step (3) CVD-coated graphene involves the synthesis of graphene by catalytic cracking of acetylene in a multi-station tubular reactor. First, a quartz boat containing 1-3g of iron-cobalt ferrite CoFe2O4 nanoparticles is placed in a quartz tube and heated to 350-450℃. Then, acetylene with a volume fraction of 99.9-99.99% is introduced at a flow rate of 25-45mL / min and reacted for 1-3h. Next, the temperature is appropriately increased to 600-700℃, and the product is kept at this temperature in an argon atmosphere for 2-3h. Then, the reaction system is slowly cooled in an argon atmosphere until it reaches a temperature of 300-350℃. The argon gas source is then turned off, and the reaction system is slowly cooled to room temperature in the air. The product is collected, soaked in hydrochloric acid for 1-2h, and then rinsed with deionized water to obtain graphene-coated nano-magnetic CoFe2O4@C particles.
5. The preparation process of an electromagnetic protective magnetic health care fabric according to claim 4, characterized in that: Step (4) involves preparing nano-magnetic CoFe2O4@C fibers by electrospinning. This includes taking 2-3g of nano-magnetic CoFe2O4@C particles, ultrasonically dispersing them in 20-30mL of polyvinylpyrrolidone (PVP), and preparing a spinning solution by magnetic stirring for 2-3h. The spinning solution is then sprayed out of the spinneret through an electrostatic nozzle and enters a high-voltage electrostatic field, eventually depositing in a collector to become nano-magnetic CoFe2O4@C fibers. The main parameters are: spinneret specification: SPN1500×0.12 mm, and spinning speed: 10-20 cm / s.
6. The preparation process of an electromagnetic protective magnetic health care fabric according to claim 5, characterized in that: Step (5) Spinning and weaving: The prepared nano-magnetic CoFe2O4@C fiber bundles are processed into electromagnetic protective and health care fabrics through wool, carding, drawing, roving, spinning, winding and weaving processes. The main parameters in the process are: blending ratio 30:30~60:60, repeated 2~3 times, blending weight 3~4 g / m, number of rovings 4~8, roving weight 0.3~1.0 g / m, and spinning weight 1~2 g / 100 m.
Citation Information
Patent Citations
Preparation method of graphene coating metal base composite powder through vapour deposition
CN106077622A
Electromagnetic wave absorbing composite textile fabric and preparation method
CN111172744A